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Isolation and single crystal study of [Nb2(μ-OMe)2(OiPr)8]. Can alcohol interchange provide the homoleptic niobium isopropoxide?

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Abstract

Niobium isopropoxide, Nb(OiPr)5, is an attractive precursor of simple and complex niobium oxides in sol-gel technology. This compound cannot, unfortunately, be obtained by alcohol interchange starting from linear chain homologues such as Nb(OMe)5 or Nb(OEt)5. The equilibrium in the latter reaction favours formation of mixed-ligand complexes, [Nb2(OR)2(OiPr)8], R = Me, Et. In particular, [Nb2(OMe)2(OPri)8] (1) has been isolated in high yield from repeated treatment of Nb2(OMe)10 with excess of isopropanol. The X-ray single crystal study reveals a dinuclear structure containing a pair of edge-sharing octahedra with methoxide ligands in the bridging position. Infrared (IR) and mass spectroscopy (MS) studies confirmed the incomplete ligand substitution. The 1H-NMR spectra suggest equilibrium between different molecular forms in solution. Solvothermal interaction of 1 with La chips in toluene/isopropanol media results in formation of a mixture of LaNb2(OiPr)13 and La2Nb4(μ4−O)4(OH)2(μ−OiPr)8(OiPr)8 (2).

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Acknowledgements

The authors are grateful to Mr. Suresh Gohil for the EI-mass spectrometry analyses and to Dr. Regine Herbst-Irmer from the Department of Structural Chemistry, University of Göttingen, for the help in the refinement of the structure of 2. This work has been supported by The Swedish Research Council. G.G. Nunes thanks also CAPES (Coordenação de Pessoal de Nível Superior-Brazil) for the grant (Process number 0481050).

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  1. Department of Chemistry, SLU, P.O. Box 7015, 75007, Uppsala, Sweden

    Giovana G. Nunes, Gulaim A. Seisenbaeva & Vadim G. Kessler

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  1. Giovana G. Nunes
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  2. Gulaim A. Seisenbaeva
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  3. Vadim G. Kessler
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Correspondence to Vadim G. Kessler.

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Nunes, G.G., Seisenbaeva, G.A. & Kessler, V.G. Isolation and single crystal study of [Nb2(μ-OMe)2(OiPr)8]. Can alcohol interchange provide the homoleptic niobium isopropoxide?. J Sol-Gel Sci Technol 43, 105–109 (2007). https://doi.org/10.1007/s10971-007-1568-0

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